1、Designation: D4527 99 (Reapproved 2016)D4527 18Standard Test Method forCarbon BlackSolvent Extractables1This standard is issued under the fixed designation D4527; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the procedure for measuring carbon black solvent extractables.1.1.1 This test method determines the to
3、tal material extracted from carbon black by toluene under specified conditions. Theprocedure is also applicable to other solvents such as cyclohexane, etc.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard d
4、oes not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. For a
5、specific precautionary statement, see Section 7.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the W
6、orld Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3051D4483 Practice for Carbon BlackStating the Precision of ASTM Test MethodsEvaluating Precision for Test MethodStandards in the Rubber and Carbon Black Manufacturing Industries (Withdraw
7、n 1990)D3396 Practice for Carbon Black Measuring the Precision of ASTM Test Methods (Withdrawn 1990)33. Summary of Test Method3.1 A specimen of carbon black is extracted for 48 h (or other specified time) in a Soxhlet extractor, the solvent removed bycontrolled temperature evaporation, and the extra
8、cted residue determined gravimetrically. If the carbon black extractables are tobe subjected to additional analysis, see Section 7.4. Significance and Use4.1 The carbon black extract test procedure provides a uniform and precise method for the gravimetric determination oforganic-solvent extractables
9、 on carbon black.Accuracy and precision are acceptable for most specification or regulatory purposes,or both. However, carbon black with very low extract (less than 0.02 %) may require a more rigorous extraction procedure. Theactual chemical composition of the extract can vary significantly with the
10、 type and origin of the carbon black.5. Apparatus5.1 Soxhlet Extraction Apparatus, with interchangeable ground joints, 40 mm I.D. extraction tube, and 250-cm3 flask.35.2 Extraction Thimble, glass, 35-mm diameter by 90-mm height, with coarse porosity fritted disc.4 When filled with 50 cm3of toluene,
11、drainage time for the first 40 cm3 should not exceed 95 s. Discard thimbles taking longer.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon BlackComponents of Carbon Black.Current edition approved
12、June 1, 2016June 1, 2018. Published July 2016July 2018. Originally approved in 1985. Last previous edition approved in 20112016 asD4527 99 (2011).(2016). DOI: 10.1520/D4527-99R16.10.1520/D4527-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at
13、serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Fisher Scientific No. 9-556B available from Fisher Scientific Co., 203 FisherAve., Pittsburgh, PA15219, has been found satisfactory. The use of Kontas K-586100 (gl
14、assjacketed) available from Kontas Glass Co., 8000 Spruce St., Vineland, NJ 08360, simplifies insulating the apparatus and reduces the possibility of breakage.4 Fisher Scientific 9-653B available from Fisher Scientific Co., has been found satisfactory.This document is not an ASTM standard and is int
15、ended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the curr
16、ent versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Heater, for extraction flask, with adjustable heat input. A hot plate extraction heater or h
17、emispherical heating mantle ispreferred.5.4 Filter Funnel, glass fritted disc type, with medium porosity fritted disc.5.5 Filter Flask, 125 or 250 cm3.5.6 Water Bath, or other suitable warming means for evaporating solvent from extract at a controlled temperature of 40 to 50C.5.7 Container, suitable
18、 for final solvent removal and weighing of residue. A lightweight aluminum dish 63 by 17.5 mm, aTFE-fluorocarbon cup or a 50-cm3 glass beaker is suggested.55.8 Vacuum Oven, gravity-convection type, capable of temperature regulation within 61C at 125C and temperatureuniformity within 65C.5.9 Oven, gr
19、avity-convection type, capable of temperature regulation within61C at 125C and temperature uniformity within65C.5.10 Desiccator.5.11 Analytical Balance, with a sensitivity of 60.1 mg.6. Reagents and Materials6.1 Toluene, having a residue after evaporation less than 10 ppm (preferably less than 2 ppm
20、).66.2 Nitrogen.6.3 Glass wool, extracted with toluene, air-dried, followed by drying in a convection oven at 125C for 1 h. Store in a closedcontainer until ready to use.6.4 Aluminum Foil.7. Precautions7.1 For safety reasons, conduct the extraction and solvent evaporation in an approved fume hood. C
21、arbon blacks may containpolynuclear aromatic compounds, some of which are carcinogens. These compounds, when present, are so strongly bound to thecarbon black that they are biologically inactive. However, they may be removed by extraction with toluene or other appropriatesolvents. Avoid skin contact
22、 with solvent extracts from such carbon blacks.7.2 For most pelleted blacks, the depth of 60 mm in the thimble should provide a sample of 15 to 25 g. Unpelleted blacks shouldbe predensified sufficiently that this depth will require a sample of at least 10 g.7.3 Do not use joint lubricant on the grou
23、nd joints. To minimize vapor loss by leakage, the joints may be sealed withTFE-fluorocarbon inserts or wrapped with TFE-fluorocarbon laboratory tape.7.4 New thimbles should be washed before use by suction with hot HCl and then rinsed with distilled or deionized water toremove loose particles of fore
24、ign matter such as dust. Thimbles are conveniently cleaned by back washing under suction withappropriate media (water, acetone, etc.). If the fritted disc becomes fouled with carbon black, it may be necessary to burn it outby slowly heating the thimble from room temperature to 500C in a muffle furna
25、ce. One hour is usually sufficient. The use ofchromic acid cleaning solution is not recommended. The permeability of the clean thimble should be checked periodically. Discardthimbles with drainage times exceeding the 95 s specified under 5.2.7.5 To prevent contamination, it is recommended that all g
26、lassware used in this procedure be reserved for the extraction ofcarbon black. If this is not feasible, the glassware must be extracted before use in accordance with 7.6.7.6 New glassware, including thimbles, must be extracted, repeatedly if necessary, with toluene or other solvent until the blankis
27、 acceptable (preferably less than 0.3 mg/150 cm3 solvent).7.7 Two or three glass beads may be added to the extraction flask to promote smooth boiling. Do not use porous boiling chips.7.8 An extraction must be discarded if there is any visible carbon black in the extraction flask or if the thimble do
28、es not drainproperly and overflows at any time during the extraction.7.9 The nitrogen should be delivered through a glass or metal tip. Do not allow plastic or rubber to contact the solvent.7.10 To protect from dust, a loose cover over the evaporation vessel is recommended.5 Fisher Scientific No. 8-
29、732-5C (aluminum dish) available from Fisher Scientific Co., and Ventron No. 2034 (teflon cup) available from Ventron Instrument Corp., CahnDivision, 16707 S. Carmenita Rd., Cerritos, CA 90701, have been found to be satisfactory.6 Distilled-in-glass toluene available from Burdick and Jackson, 1953 T
30、.S. Harvey, Muskegan, MI 49442 and Photrex grade available from J.T. Bauer Chemical Co., 223Red School Ln., Phillipsburg, NJ 08865 are preferred products. Analytical reagent grade available from Mallinckrodt, Inc., 675-T McDonnell Blvd., St. Louis, MO 63134has generally been found acceptable.D4527 1
31、827.11 Solvent evaporation may be conducted in a vacuum evaporator, if available.7.12 Any further analysis of the extracted material typically requires that it be in solution. Complete re-solution of the dryextract may be difficult or impossible. Therefore, if further analysis is to be performed, an
32、 additional sample of the carbon blackshould be extracted and solvent removal carried only to the desired reduced volume. It is recommended that exposure to stronglight, especially sunlight, be avoided during extraction and subsequent handling, and that the extract be blanketed with inert gas(nitrog
33、en) if retained for any length of time.7.13 It has been found that there may be significant variation in the amount of residue found in different bottles of toluenebearing the same lot number. Consequently, blanks should be run on each bottle.8. Procedure8.1 Dry an adequate specimen of the carbon bl
34、ack for 1 h in the gravity-convection oven set at 125C in an open container ofsuitable dimensions so that the depth of the black is no more than 10 mm. Cool and store the sample in a desiccator.8.2 Weigh, into a clean, dry extraction thimble, sufficient dried carbon black to fill the thimble to a de
35、pth of approximately 60mm. Record the weight of black to 0.1 g. Place a plug of glass wool above the black. Insert the thimble into the extraction tube,place 150 cm3 of toluene in the extraction flask, and assemble the apparatus (see 7.1 7.6).8.3 Extract continuously for 48 h (or other time if speci
36、fied), heating so that the cycle time between siphonings is 4 to 5 min(see 7.7). Wrap aluminum foil loosely around the extraction tube and upper part of the flask to reduce heat loss. Terminate theextraction with the extraction cup nearly full to reduce the quantity of solvent to be subsequently eva
37、porated from the residue inthe extraction flask (See 7.8).8.4 Filter the contents of the extraction flask into a clean filter flask using moderate suction, rinsing the extraction flask and filterfunnel with several small portions of toluene.8.5 Evaporate the contents of the filter flask at 40 to 50C
38、 until approximately 10 cm3 remains. Direct a stream of dry nitrogenonto the surface of the solution to hasten evaporation (see 7.9 7.11).8.6 Transfer the remaining solution to the previously dried and weighed (to 0.1 mg) final container, rinsing the flask with severalsmall portions of toluene. Cont
39、inue evaporation to essentially dryness (see 7.12).8.7 To complete solvent removal to constant residue mass, place the container in a vacuum oven at 40C. Setting the containeron the floor of the oven should be avoided; a non-conductive support or equivalent should be used. Slowly reduce the oven pre
40、ssureto approximately 3.3 kPa and thereafter hold at that level. After a suitable time (usually 45 min to 1 h), cool the container andcontents to room temperature in a desiccator and weigh to 0.1 mg. Return to the oven for 15 min, cool, and reweigh. Repeat asnecessary until the mass is constant. Sub
41、tract the original mass to obtain the mass of residue.8.8 Make duplicate blank determinations on each bottle of toluene placed in use. Follow this procedure exactly but omit thecarbon black (see 7.13).9. Calculation9.1 Calculate the mass percent extractables to the nearest 0.01 % as follows:Extracta
42、bles,mass%5 R2BW 3100 (1)where:R = mass of residue, g,B = mass of residue from blank, g, andW = mass of carbon black sample, g.10. Report10.1 Report the following information:10.1.1 Proper identification of the sample,10.1.2 The solvent used,10.1.3 The extraction time, and10.1.4 The result obtained,
43、 reported to the nearest 0.01 %.11. Precision and Bias11.1 These precision statements have been prepared in accordance with Practice D4483-99. Refer to this practice forterminology and other statistical details.11.2 A type 1 inter-laboratory precision program was conducted as detailed in Table 1 and
44、 Table 2. Extraction times were 48h or 16 h, respectively. Both repeatability and reproducibility represent short term (daily) testing conditions. The testing wasD4527 183performed using one operator in each laboratory performing the test once on two different days. A test result is the value obtain
45、edfrom a single determination. Acceptable difference values were not measured.11.3 These precision data are based on single tests of three samples by five laboratories on two days. The range of the samplesstudied was from about 0.06 % to about 1.02 %.The results of the precision calculations for thi
46、s test are given in Table 1Precisionand Table 2is expressed in absolute terms The materials are arranged in descending “mean level” order. The preferredprecision is shown in bold text.NOTE 1The precision is based on limited data in that only five laboratories participated in the interlaboratory stud
47、y.11.4 RepeatabilityIn The pooled absolute repeatability, r,test method statistical terminology, bias is the of this test has beenestablished as 0.04 % for 48 h extraction time and as 0.03 % for 16 h extraction time. Any other value in Table 1 or Table2difference between an average test value and th
48、e reference or true test property value. Reference values do not exist may be usedas an estimate of repeatability, as appropriate. The difference between two single test results (or determinations) found on identicaltest material under the repeatability conditions prescribed for this test method sin
49、ce the value will exceed the repeatability on anaverage of not more than once in 20 cases in the normal and correct operation of the method. Two single test results that differby more than the appropriate value from Table 1 or levelTable 2 of the test property is exclusively defined by this test method.Bias, therefore, cannot be determined.must be suspected of being from different populations and some appropriate action taken.NOTE 1Appropriate action may be an investigation of the test method procedure or apparatus for faulty operation or the declaration of
